Development of a method for the determination of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone in dust using liquld chromatography tandem mass spectrometry

LC-MS/MS를 이용하여 먼지 속의 NNK (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone) 정량 분석법 개발

  • Received : 2015.01.16
  • Accepted : 2015.02.06
  • Published : 2015.02.25


4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), a tobacco specific nitrosamine found only in tobacco products. The ability to monitor biomarker concentrations is very important in understanding environmental tobacco smoke (ETS). In this study, an efficient and sensitive method for the analysis of NNK in dust was developed and validated using liquid chromatography tandem mass spectrometry. Dust was collected with filter paper soaked in methanol. The standard solution and dust sample were diluted with 100 mM ammonium acetate and extracted using dichloromethane. Our calibration curves ranged from 25 to $10^4pg/mL$. Excellent linearity was obtained with correlation coefficient values between 0.9996 and 1.0000. The limit of detection (LOD) was 5 pg/mL ($S/N{\geq}3$) and the retention time was 10 min. The limit of quantification (LOQ) was 25 pg/mL, and the acceptance criteria was the rate of 98-103% (80-120% at levels up to $3{\times}LOQ$). The coefficient of variations (CV) was 2.8%. Accuracies determined from dust samples spiked with four different levels of NNK racurves ranged that from 25 to 104 pg/mL. Excellent linearity was obtained between 92.1% and 114%. The precision of the method was acceptable (5% of CV). The recovery rates of the whole analytical procedure at low, medium, and high levels were 105.7-116.5% for NNK. The carry-over effects during LC-MS/MS analysis were not observed for NNK. This manuscript summarizes the scientific evidence on the use of markers to measure ETS.


4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) Environmental tobacco smoke (ETS) Tobacco-specific nitrosamines (TSNAs) LC-MS/MS Dust


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Supported by : National Cancer Center